CN207816917U - Gas-chromatography-ion mobility spectrometry detector and combined apparatus - Google Patents
Gas-chromatography-ion mobility spectrometry detector and combined apparatus Download PDFInfo
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- CN207816917U CN207816917U CN201721895694.5U CN201721895694U CN207816917U CN 207816917 U CN207816917 U CN 207816917U CN 201721895694 U CN201721895694 U CN 201721895694U CN 207816917 U CN207816917 U CN 207816917U
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Abstract
A kind of gas-chromatography ion mobility spectrometry detector and combined apparatus, gas-chromatography ion mobility spectrometry detector include gas-chromatography mechanism and ion mobility spectrometry mechanism.Gas-chromatography mechanism includes chromatographic column and injection port.Ion mobility spectrometry mechanism includes migration tube and connector, and the metal terminal pad of connector includes chromatography metal dish, Ion transfer metal dish and semi-permeable membrane;Ion transfer sample introduction carrier gas inlet, Ion transfer sample cavity and sample feeding mouth are provided on Ion transfer metal dish;Chromatographic sample chamber and Ion transfer sample cavity are separated by semi-permeable membrane.Chromatography column feed materials carrier gas enters via injection port in chromatographic column, enter chromatographic sample chamber through chromatographic sample carrier gas inlet, sample molecule of the part through chromatography column feed materials carrier gas load can be through in semipermeable membrane to Ion transfer sample cavity, and enters migration tube through sample feeding mouth;The chromatography column feed materials carrier gas of another part sample and whole does not penetrate into Ion transfer sample cavity, is discharged by chromatographic sample chamber and chromatography outlet port.
Description
Technical field
The utility model belongs to technical field of analysis and detection, more particularly to a kind of gas-chromatography and ion mobility spectrometry (GC-
IMS method and apparatus associated with).
Background technology
Ionic migration spectrometer (IMS) is widely used in the feature that simple in structure, high sensitivity, analyze speed wait soon
The detection or monitoring of chemical warfare agent, drugs, explosive, environment etc..But IMS is separately as detecting instrument to complicated component
When sample is detected, there are the following problems:(1) due to manufacturing process the problem of, the resolution ratio of existing commercialization IMS is 40
Left and right, therefore be difficult to be distinguished to substance similar in mobility;(2) in ionized region complexity can occur for the ion of some compounds
Reaction and bury in oblivion mutually;(3) dynamic range of IMS is relatively low, can shadow when there is one or more of compound concentrations very big
The ion for ringing other compounds generates, to cause missing inspection.Based on the above reason IMS when detecting the sample of complicated component, hold
It easily fails to report, report by mistake.
Gas chromatograph is current universally recognized high efficiency and high stability separating tool, in the separation point of gaseous substance
It is widely used in analysis.However, selectivity and sensitivity difference of the different detectors to substance, or even the detector having is not
It is common detector such as electron capture detector and hydrogen flame detector, in addition thermal conductivity detector (TCD) is as common detector,
The detection limit that its sensitivity can not fully meet many substances requires.
It is outstanding to complex sample that GC is not only effectively utilized in gas-chromatography-ion mobility spectrometry (GC-IMS) joint technology
Separating capacity, while being also effectively utilized that IMS detector sensitivities are high and positive and negative double mode is wide to the selectivity of substance
Feature, this joint technology can greatly improve the accuracy of detection and detection sensitivity to mixture.Therefore, combination in recent years
Technology has obtained enough attention and swift and violent development in analysis detection field.
However, in existing GC-IMS joint technology, or the connection type between GC and IMS is that chromatographic column is direct
It is inserted in the ionized region front end of IMS or is chromatographic column to be directly inserted in the ionized region of IMS, or chromatographic column is inserted in IMS
Reaction zone in, these connection types usually it is simple and easy to operate.But this kind of connection type on the one hand can be in the long-term of instrument
Pollution is generated to migration tube inside during use and is difficult to clear up, on the other hand since the reactive ion of IMS holotypes is main
It is that the reactive ion of negative mode is mainly and the high pure nitrogen as GC carrier gas continues into IMS also and can influence the ionization ring of IMS
Border makes holotype reactive ion complicated component, and negative mode is difficult to generate these factors such as reactive ion and is all unfavorable for GC-IMS's
Long-time stability and popularization.
Utility model content
One main purpose of the utility model is to overcome at least one defect of the above-mentioned prior art, provides a kind of gas
Phase chromatography-ion mobility spectrometry detector and combined apparatus, to migration tube inside during the long-time service to solve existing instrument
It leads to the problem of pollution and is difficult to clear up.
To reach above-mentioned purpose, the utility model provides a kind of gas-chromatography-ion mobility spectrometry detector comprising gas phase
Chromatography mechanism and ion mobility spectrometry mechanism.
Gas-chromatography mechanism includes chromatographic column and injection port, and injection port is located at one end of chromatographic column, and is connected to chromatographic column.
Ion mobility spectrometry mechanism includes migration tube and connector, connector connection be set to chromatographic column and migration tube it
Between, connector includes metal terminal pad, metal terminal pad include the chromatography metal dish being correspondingly arranged and Ion transfer metal dish and
Semi-permeable membrane between chromatography metal dish and Ion transfer metal dish, chromatography metal dish are provided with chromatographic sample carrier gas inlet, chromatography
Sample cavity and chromatography outlet port, chromatographic sample carrier gas inlet are connected to chromatographic column and chromatographic sample chamber;Ion transfer metal
Be provided with Ion transfer sample introduction carrier gas inlet, Ion transfer sample cavity and the sample feeding mouth of connection on disk, sample feeding mouth with
Migration tube is connected to;Chromatographic sample chamber and Ion transfer sample cavity are separated by semi-permeable membrane.
Wherein, sample molecule, which enters under chromatography column feed materials carrier gas effect via injection port, carries out pre-separation in chromatographic column, pass through
The sample molecule of pre-separation enters chromatographic sample chamber through chromatographic sample carrier gas inlet, and a part of sample molecule can be oozed through semi-permeable membrane
It arrives in Ion transfer sample cavity thoroughly, and enters migration tube through sample feeding mouth;Another part sample and the chromatography column feed materials of whole carry
Gas is discharged after through chromatography outlet port.
According to an embodiment, injection port is shunting or Splitless injecting samples mouth.
According to an embodiment, chromatographic column is capillary chromatograph or boundling capillary column, and gas-chromatography mechanism further includes chromatographic column
Set, for protecting chromatographic column and being evenly heated to chromatographic column, and chromatography column sleeve make chromatographic column and injection port and with migration tube it
Between be tightly connected.
According to an embodiment, migration tube includes holotype pipe and negative mode pipe, and is connected to by connector.
According to an embodiment, connector further includes high-temperature insulation disk, is set to the both sides of metal terminal pad, and metal
Terminal pad is grounded.
According to an embodiment, chromatography metal dish, Ion transfer metal dish and semi-permeable membrane use O-ring seals and screw assemblies
Sealing is fixed, and chromatographic sample chamber and Ion transfer sample cavity are two independent sealed toroidal cavities.
Further include heating film, heat-preservation cotton and shielding case according to an embodiment, heating film coat injection port, chromatography column sleeve and
Migration tube;Heat-preservation cotton coats the outside of heating film;Shielding case is set between migration tube and heating film.
The utility model also provides a kind of gas-chromatography-ion mobility spectrometry combination device, including air-channel system and above-mentioned
Gas-chromatography-ion mobility spectrometry detector, wherein air-channel system includes chromatography gas circuit, the first migration gas circuit and the second migration gas
Road, chromatography gas circuit are connected to injection port, and chromatography column feed materials carrier gas can enter chromatographic column via chromatography gas circuit and injection port, a part
Sample molecule can be through in semipermeable membrane to Ion transfer sample cavity;First migration gas circuit both ends respectively with migration tube and;
Second migration gas circuit is connected to migration tube, for providing migration gas to migration tube;Gas energy is discharged by the migration tube of migration tube discharge
It is enough to enter transference tube via the first migration gas circuit, the second migration gas circuit and Ion transfer sample introduction carrier gas inlet, and by chromatography
Sample cavity penetrate into the sample in Ion transfer sample cavity can under the action of migrating sample introduction carrier gas via sample feeding mouth into
Enter ionization in migration tube, and reaches Faraday plate under the action of migrating electric field and be detected.
According to an embodiment, chromatography gas circuit includes filter, combination valve and flow controller, and chromatography column feed materials carrier gas can be through
Injection port is entered by filter, combination valve and flow controller.
According to an embodiment, migration tube includes holotype pipe, negative mode pipe, positive discharge gas interface and bears discharge gas interface,
Holotype pipe is connected to negative mode pipe by connector, and gas interface is just being discharged and is being connected to holotype pipe, is born discharge gas interface and is born
Pattern pipe is connected to;Air-channel system further includes buffering bottom plate, and buffering bottom plate includes the first cushion chamber and the second cushion chamber, the first buffering
Chamber is connected between positive discharge gas interface and the first migration gas circuit, and the second cushion chamber is connected to negative discharge gas interface and the first migration
Between gas circuit.
According to an embodiment, the first migration gas circuit includes the first branch, the second branch and the third branch connected by threeway
Road, the migration sample introduction carrier gas from the first cushion chamber and the second cushion chamber converge in the first branch, and the second branch is equipped with molecule
Sieve, and be connected to Ion transfer sample introduction carrier gas inlet, third branch road is equipped with clarifier and miillpore filter, from the first branch
A part for migration sample introduction carrier gas enters the second branch, and another part enters third branch.
According to an embodiment, for buffering bottom plate including further including third cushion chamber, the first migration gas circuit further includes the 4th branch,
The second branch is connect with third cushion chamber, the 4th branch connection third cushion chamber and Ion transfer sample introduction carrier gas inlet, the 4th
Road is equipped with flow controller.
According to an embodiment, the second migration gas circuit includes holotype branch and negative mode branch, and holotype branch is connected to
Between third cushion chamber and holotype pipe, negative mode branch is connected between third cushion chamber and negative mode pipe.
Further include circuit according to an embodiment, circuit includes power module, mainboard, preceding amplification module, high-pressure modular, heating
Module and control module, mainboard are used for connection migration pipe outgoing cable, and for being preceding amplification module, high-pressure modular, control panel
Slot is provided;Preceding amplification module is used to carry out shaping, filtering and amplification to Faraday plate received signal;High-pressure modular be used for for from
Cervical orifice of uterus provides saltus step pulse, provides electric field for migration area and for grid-disk;Heating module is for being heated;Control module is used
In modification and control of the realization to heating and gas-chromatography-ion mobility spectrometry detector start and stop.
Further include shielding shell according to an embodiment, it includes migration tube heat shielding shell, Faraday plate shielding cylinder,
Migration tube bulk shielding shell and high pressure and the shielding shell before put.
The advantageous effect of the utility model compared to the prior art is:Gold is set as in the middle part of the connector of the utility model
Belong to terminal pad, and be provided with semi-permeable membrane in metal terminal pad, semi-permeable membrane only allows the part sample through gas-chromatography organizational separation
Product enter the detection of ion mobility spectrometry mechanism, and high-purity carrier gas is prevented outside semi-permeable membrane, not only ensure that ion mobility spectrometry mechanism
Independent ionization environment is unaffected, and can greatly simplify gas-chromatography-ion mobility spectrometry detector and process is used for a long time
The cleaning of intermediate ion migration spectrum detector portion;Also, the rear end of metal terminal pad is provided with chromatography outlet port, thus
It can prevent that certain toxic samples are expelled directly out and injury is generated to personnel and environment.Efficiently solving the long-term of existing instrument makes
It is difficult to clear up with pollution is led to the problem of to migration tube inside in the process.
Description of the drawings
Consider the detailed description of the following preferred embodiment to the utility model in conjunction with the accompanying drawings, the utility model it is each
Kind target, feature and advantage will become apparent.Attached drawing is only the exemplary diagram of the utility model, is not necessarily
It is drawn to scale.In the accompanying drawings, same reference numeral always shows same or similar component.Wherein:
Fig. 1 is the structural schematic diagram of the gas-chromatography-ionic migration spectrometer combined apparatus of the utility model;
Fig. 2 is the metal terminal pad structural schematic diagram of the gas-chromatography-ionic migration spectrometer combined apparatus of the utility model;
Fig. 3 is the air-channel system schematic diagram of the gas-chromatography-ionic migration spectrometer combined system of the utility model;And
Fig. 4 is the gas-chromatography-ionic migration spectrometer combined system of the utility model to buffer the complete machine that bottom plate is support
Forward sight layout.
Specific implementation mode
Example embodiment is described more fully with reference to the drawings.However, example embodiment can be with a variety of shapes
Formula is implemented, and is not understood as limited to embodiment set forth herein;On the contrary, thesing embodiments are provided so that this practicality is new
The design of example embodiment more comprehensively and completely, and is comprehensively communicated to those skilled in the art by type.It is identical in figure
Reference numeral indicates same or similar structure, thus will omit their detailed description.
The term of relativity, such as " relatively low " or " bottom " and " higher " or " top " may be used in embodiment, to retouch
State relativeness of the component for another component of icon.It is appreciated that, if the device overturning of icon made thereon
Lower reverse, then the component described in " relatively low " side will be as in the component of " higher " side.In addition, when certain layer in other layers or
When substrate "upper", it is possible to refer to " direct " on other layers or substrate, or refer to certain layer on other layers or substrate, or refer to other
The other layers of sandwiched between layer or substrate.
The utility model provides a kind of gas-chromatography-ion mobility spectrometry detector 100 and the gas phase color comprising the detector
Spectrum-ion mobility spectrometry combination device.As shown in Figure 1, 2, gas-chromatography-ion mobility spectrometry detector 100 includes gas-chromatography machine
Structure and ion mobility spectrometry mechanism.
Gas-chromatography mechanism includes chromatographic column 112 and injection port 114, and injection port 114 is located at one end of chromatographic column 112, and
It is connected to chromatographic column 112.
Ion mobility spectrometry mechanism includes migration tube 111 and connector, and connector connection is set to chromatographic column 112 and migration
Between pipe 111, connector includes metal terminal pad 110, and metal terminal pad 110 includes 137 He of chromatography metal dish being correspondingly arranged
Semi-permeable membrane 139 between Ion transfer metal dish 138 and chromatography metal dish 137 and Ion transfer metal dish 138, chromatography metal dish
137 are provided with chromatographic sample carrier gas inlet 144, chromatographic sample chamber 142 and chromatography outlet port 145, and chromatographic sample carrier gas enters
Mouth 144 is connected to chromatographic column 112 and chromatographic sample chamber 142;Be provided on Ion transfer metal dish 138 Ion transfer of connection into
Sample carrier gas inlet 146, Ion transfer sample cavity 143 and sample feeding mouth 147, sample feeding mouth 147 are connected to migration tube 111;
Chromatographic sample chamber 142 and Ion transfer sample cavity 143 are separated by semi-permeable membrane 139.
Wherein, sample molecule enters in chromatographic column 112 via injection port 114 under chromatography column feed materials carrier gas effect and is divided in advance
From pre-separated sample molecule enters chromatographic sample chamber 142 through chromatographic sample carrier gas inlet 144, and a part is by chromatography column feed materials
The sample molecule of carrier gas load can be penetrated into through semi-permeable membrane 139 in Ion transfer sample cavity 143, and through sample feeding mouth 147
Into migration tube 111;The chromatography carrier gas of another part sample molecule and whole is discharged after through chromatography outlet port 145.
It is set as metal terminal pad 110 in the middle part of the connector of the utility model, and is provided with half in metal terminal pad 110
Permeable membrane 139, semi-permeable membrane 139 only allow the sample segment through gas-chromatography organizational separation to enter the detection of ion mobility spectrometry mechanism, and
High-purity carrier gas is prevented outside semi-permeable membrane 139, not only ensure that the independent ionization environment of ion mobility spectrometry mechanism is unaffected, and
And it can greatly simplify ionic migration spectrum detection device part during gas-chromatography-ion mobility spectrometry detector 100 is used for a long time
Cleaning;Also, the rear end of metal terminal pad 110 is provided with chromatography outlet port 145, it can be with sample absorption plant
Connection, activated carbon+molecular sieve can be used in sample absorption plant, thus can prevent certain toxic samples be expelled directly out and to personnel
And environment generates injury.Sample introduction residual is accumulated inside to migration tube 111 during efficiently solving the long-time service of existing instrument
It leads to the problem of pollution and is difficult to clear up.
In the present embodiment, injection port 114 is shunting or Splitless injecting samples mouth 114.
Chromatographic column 112 can be that capillary chromatograph or boundling capillary column (MCC), this case are illustrated by taking MCC columns as an example.Gas phase
Chromatography mechanism further includes chromatography column sleeve 113, and for protecting chromatographic column 112 and being heated to chromatographic column 112, chromatography column sleeve 113 makes
It chromatographic column 112 and injection port 114 and is tightly connected between migration tube 111.
Chromatography metal dish 137, Ion transfer metal dish 138 and semi-permeable membrane 139 are sealed using O-ring seals and screw assemblies
Fixed, it is empty that chromatographic sample chamber 142 and Ion transfer sample cavity 143 can be divided into two independent sealed annulars by semi-permeable membrane 139
Chamber.
The present embodiment is covered with heating film in the part of the needs such as injection port 114, chromatography column sleeve 113 and migration tube 111 heating
107, and heat-preservation cotton 104 is covered with outside heating film 107.To prevent heating film 107, external electromagnetic field etc. to 111 signal of migration tube
Influence, the aluminum hull 108 for being coated with high temperature resistant and high insulating cement using inner wall between migration tube 111 and heating film 107 shielded.For
The anti-interference ability for improving Faraday plate 101 is shielded in 101 outside of Faraday plate using metal dish 102.
The utility model also provides a kind of gas-chromatography-ion mobility spectrometry combination device, including air-channel system and above-mentioned
Gas-chromatography-ion mobility spectrometry detector 100, below illustrates its concrete structure and operating method.
As shown in figure 3, air-channel system include chromatography gas circuit, first migration gas circuit and second migration gas circuit, chromatography gas circuit with
Injection port 114 is connected to, and chromatography column feed materials carrier gas can enter chromatographic column 112, a part of sample via chromatography gas circuit and injection port 114
Molecule can be penetrated into through semi-permeable membrane 139 in Ion transfer sample cavity 143;First migration gas circuit both ends respectively with migration tube
111 Hes;Second migration gas circuit is connected to migration tube 111, for providing migration gas to migration tube 111;It is discharged by migration tube 111
Migration tube be discharged gas can via first migration gas circuit, second migration gas circuit and Ion transfer sample introduction carrier gas inlet 146 enter from
Sub- migration tube, and penetrating into the sample in Ion transfer sample cavity by chromatographic sample chamber can be in the work of Ion transfer sample introduction carrier gas
Under via sample feeding mouth 147 enter migration tube 111 in ionization, and under the action of migrate electric field arrival Faraday plate and by
Detection.
Wherein, chromatography gas circuit includes filter 116, combination valve 117 and flow controller 118, and chromatography column feed materials carrier gas can
Enter injection port 114 via filter 116, combination valve 117 and flow controller 118.
Migration tube 111 is preferably integrated ceramic migration tube, and can be designed as having single detection pattern according to needs
Monotype migration tube or with the two-tube of positive and negative two detection patterns.In this case, migration tube 111 includes holotype pipe, negative norm
Formula pipe, positive discharge gas interface 106 and negative discharge gas interface 105, holotype pipe is connected to negative mode pipe by connector, positive to be discharged
Gas interface 106 is connected to holotype pipe, and negative discharge gas interface 106 is connected to negative mode pipe.
Meanwhile to ensure that insulation between 111 positive and negative pattern of migration tube and reduction interfere with each other, connector further includes resistance to
High-temperature insulation disk 109 is set to the both sides of metal terminal pad, uses high temperature resistant, good insulating and the small cause of the coefficient of expansion
Close proximate matter material makes, such as PTFE, PEEK, ceramics etc., and stainless steel making, and metal terminal pad 110 can be used in metal terminal pad 110
Ground connection.
Air-channel system further includes buffering bottom plate 120, and buffering bottom plate 120 includes cushion chamber A and cushion chamber B, cushion chamber A connections
Between just discharge gas interface 106 and the first migration gas circuit, cushion chamber B is connected to negative 105 and first migration gas of discharge gas interface
Between road.
Wherein, buffering bottom plate 120 can continue to use same technique in existing patent application CN 106645472A, can not only be effective
Reduction diaphragm pump valve work time pulse qi of chong channel ascending adversely stream and instrument shake influence to 111 internal gas flow of migration tube and be also beneficial to install
Debugging and repair, details are not described herein.
First migration gas circuit may include the first branch S1 connected by threeway 122, the second branch S2 and third branch S3,
Migration sample introduction carrier gas from cushion chamber A and cushion chamber B converges in first branch S1, and the second branch S2 is equipped with molecular sieve 124,
And be connected to Ion transfer sample introduction carrier gas inlet 146, third branch S3 is equipped with clarifier 116 and miillpore filter 123, from the
A part for the migration sample introduction carrier gas of one branch S1 enters the second branch S2, and another part enters third branch S3.
For buffering bottom plate 120 including further including cushion chamber C, the first migration gas circuit further includes the 4th branch S4, the second branch S2
It is connect with cushion chamber C, the 4th branch S4 connection cushion chamber C and Ion transfer sample introduction carrier gas inlet 146, the 4th branch S4 are equipped with
Flow controller 118.
Second migration gas circuit includes holotype branch S5 and negative mode branch S6, and holotype branch S5 is connected to cushion chamber C
Between holotype pipe, negative mode branch S6 is connected between cushion chamber C and negative mode pipe.
When instrument works, chromatography column feed materials carrier gas is provided by air source 115 and removes high-purity gas through the filter 116 in pipeline
In the impurity such as hydrocarbon, oxygen and water, then enter instrument gas circuit through the fixed combination valve 117 of casing outer wall.Wherein,
When combination valve 117 is made of two one-way seal valves, when connecting two one-way seal valves, the primary and secondary head spool of one-way seal valve
Mutually open-top, combination valve 117 forms access, each self-closing of two one-way seal valves when disconnection.Wherein, in the injection port of instrument 114
Front end regulates and controls chromatography column feed materials carrier gas using flow controller 118, obtains the chromatography column feed materials carrier gas of regulation and control from injection port 114
Chromatography carrier gas inlet it is preheated after enter vaporizer and the indoor test sample that will gasify and bring into chromatographic column 112 and divided in advance
From (reference numeral 119 indicates gas-chromatography mechanism in Fig. 3), the sample through MCC pre-separations is again from the chromatography of intermediate connecting body gold
The chromatographic sample carrier gas inlet 144 for belonging to terminal pad 137 enters chromatographic sample chamber 142 and penetrates into Ion transfer through semi-permeable membrane 139
In sample cavity 143, then under the action of Ion transfer sample introduction carrier gas through sample feeding mouth 147 again through ionization area, reaction zone, from
Cervical orifice of uterus simultaneously reaches Faraday plate under the action of migrating electric field and is detected.And do not penetrate into Ion transfer sample cavity 143 in time
Interior sample will be adsorbed with chromatography carrier gas together by chromatographic sample chamber 142 through chromatography outlet port 145 using filter 116
It is discharged from exhaust piping after absorption.
It is this in such a way that semi-permeable membrane 139 is isolated by chromatography with ion mobility spectrometry, on the one hand can ensure that ion moves
The ionization environment of shifting is not influenced by chromatography carrier gas;On the other hand the cleaning of ion mobility detector part can also be simplified.
In gas circuit connection, buffering bottom plate 120 is made of duralumin, and has 3 independent sealed cavitys, i.e., above-mentioned buffering
Chamber A, cushion chamber B and cushion chamber C.
The discharge gas interface 105 of negative mode is connected with the suction interface of diaphragm pump 121 again after being connected with cushion chamber B;Holotype
The discharge gas interface 106 of formula is connected with the suction interface of diaphragm pump 121 again after being connected with cushion chamber C.Positive negative mode discharge gas exists
Converge at threeway 122, is connected with Ion transfer purification molecular sieve 124 one of in other two channels of threeway 122, separately
One is connected with clarifier 116, and 116 end of clarifier is provided with miillpore filter 123.Wherein, what is be connected with clarifier 116 is logical
Road is used for equilibrium air pressure.The channel being connect with Ion transfer purification molecular sieve 124 is for purifying Ion transfer circulating air, circulating air
Be divided into after molecular sieve 124 purifies and enters cushion chamber C three tunnels and under the control of flow controller 118 respectively with it is positive and negative
The migration gas interface 103 of pattern migration tube 111 is connected to, and is formed migration gas and is moved with the ion on Ion transfer metal dish 138
146 connection of shift-in sample carrier gas inlet forms Ion transfer sample introduction carrier gas, and Ion transfer sample introduction carrier gas will transmit through the entrance of semi-permeable membrane 139
The sample of Ion transfer sample cavity 143 introduces from sample feeding mouth 147 and carries out ionization analytics in migration tube 111.
Gas-chromatography-ion mobility spectrometry combination device further includes circuit, and circuit includes power module 127, mainboard 129, preceding
Amplification module 133, high-pressure modular 130, heating module and control module 132,129 one side of above-mentioned mainboard are used for connection migration pipe
111 outgoing cables (111 high-voltage connection of Faraday plate signal wire and migration tube), are on the other hand additionally operable to as preceding amplification module, high pressure
Module, control panel etc. provide rapid slot, are convenient for fixation, replacement and the repair of each module;Power module 127 turns for that will exchange
It is changed to direct current, and permanent steady operating voltage is provided for mainboard etc..
To reduce the vibrations that the work of diaphragm pump 121 generates, diaphragm pump 121 and the connection of buffering bottom plate 120 use beam
125 and vibration-damping screw nail.AC supply voltage can directly be mainboard 129, control mould after power module 127 is converted into DC low-voltage
Block 132, high-pressure modular 130 and preceding amplification module 134 provide permanent steady direct-current working volts.
High-pressure modular 131 is used to for ion gate provide saltus step pulse, is migration area and is that (inhibition is deleted and farad for grid-disk
Between disk) consistent electric field is provided, preceding amplification module 134 is used to carry out shaping to Faraday plate received signal, filters and put
Greatly;For control module 132 for realizing to heating and thermal insulation, instrument starts shutdown and the modification and control of other running parameters.Add
Thermal modules are used to heat the structure of GC-IMS work under the high temperature conditions;Control module is for realizing to heating, instrument
Start and stop and the modification of other running parameters and control.
Fixed column 128 is used to mainboard 129 being fixed on buffering bottom plate 120.Mainboard 129 be used for for high pressure, it is preceding put, middle control
Deng offer rapid slot;Simultaneously for the work required high pressure of migration tube 111 to be introduced migration pipe electrode and by Faraday plate signal
Amplification module carries out shaping filter and amplification etc. before being delivered to.Wherein, to avoid high pressure from existing signal and Faraday plate signal
It is interfered in transmission process, between mainboard and 111 interelectrode high-voltage connection of migration tube and Faraday plate signal and mainboard
Lead be all made of screened coaxial cable 135.
Meanwhile high-tension shielding cover 131 is also respectively adopted in high-pressure modular 130, preceding amplification module, preceding shielding case 134 of putting shields, and moves
It moves pipe 111 and is migrated 108 encirclement of the shielding aluminium of pipe 111 skin, shielded cable and shielding case can efficiently reduce outer bound pair migration tube
111 and circuit electromagnetic interference, so that detector system is worked long-term effectively.
Wherein, above-mentioned shielding shell includes the heating shielding of migration tube 111 shell, Faraday plate shielding cylinder, migration tube 111
The metallic shield of bulk shielding shell and high pressure and the shielding shell etc. before put, multilayer can effectively reduce extraneous and GC-IMS
Internal circuit collects migration tube 111 and the interference of output signal, the shielding of circuit can reduce outer bound pair circuit job stability
Interference, so that 111 module of migration tube is worked long-term effectively.
Buffering bottom plate 120 provide buffer cavity can effectively eliminate the air-flow pulse of diaphragm pump 121, and can realize just,
Negative mode migrates gas and the independent control that gas is discharged;On the other hand buffering bottom plate 120 be also molecular sieve 124 and gas-chromatography-from
The gas circuit connection of sub- migration spectrum detector 100 etc. provides fast interface, facilitates replacement, the gas circuit connection of molecular sieve.
At the same time, gas-chromatography-ion mobility spectrometry detector 100, molecular sieve 124, power module 127, heating module
126, air pump beam 125 and mainboard 129 etc. are each attached on buffering bottom plate 120 so that system can become an entirety
Buffering bottom plate 120 can directly be revealed the whole truth from tool housing 136 when module, repair and installation, or be refilled after the completion of peace tune
Enter in tool housing 136, this not only facilitates assembly, repair and replacement of the detector in casing, while also so that detector
With good antidetonation, shield effectiveness.
In conclusion the utility model provides a kind of the connecting interface method and its equipment of GC-IMS joint technology, no
It is only capable of greatly facilitating interconnection between chromatography and ionic migration spectrometer, the maintenance of GC-IMS, the cleaning of migration tube, while can also protect
The ionization environment for demonstrate,proving Ion transfer stabilization is unaffected so that the operation and maintenance of GC-IMS is more convenient, and performance is more stable.
Although exemplary embodiment describing the utility model with reference to several, it is to be understood that, term used is explanation
With term exemplary, and not restrictive.Since the utility model can be embodied in a variety of forms without departing from practical new
The spirit or essence of type, it should therefore be appreciated that above-described embodiment is not limited to any details above-mentioned, and should be in appended claims
Defined by widely explain in spirit and scope, therefore fall into whole variations and modification in claim or its equivalent scope
Appended claims are all should be to be covered.
Claims (15)
1. a kind of gas-chromatography-ion mobility spectrometry detector, which is characterized in that including:
Gas-chromatography mechanism, including chromatographic column and injection port, injection port are located at one end of chromatographic column, and are connected to chromatographic column;And
Ion mobility spectrometry mechanism, including migration tube and connector, connector connection are set between chromatographic column and migration tube, even
Junctor includes metal terminal pad, and metal terminal pad includes the chromatography metal dish being correspondingly arranged and Ion transfer metal dish and chromatography gold
Belong to the semi-permeable membrane between disk and Ion transfer metal dish, chromatography metal dish is provided with chromatographic sample carrier gas inlet, chromatographic sample chamber
And chromatography outlet port, chromatographic sample carrier gas inlet are connected to chromatographic column and chromatographic sample chamber;It is set on Ion transfer metal dish
It is equipped with Ion transfer sample introduction carrier gas inlet, Ion transfer sample cavity and the sample feeding mouth of connection, sample feeding mouth and migration tube
Connection;Chromatographic sample chamber and Ion transfer sample cavity are separated by semi-permeable membrane;
Wherein, sample molecule, which enters under chromatography column feed materials carrier gas effect via injection port, carries out pre-separation in chromatographic column, through dividing in advance
From sample molecule enter chromatographic sample chamber through chromatographic sample carrier gas inlet, a part of sample molecule can be arrived through semipermeable membrane
In Ion transfer sample cavity, and enter migration tube through sample feeding mouth;Another part sample molecule and whole chromatography carrier gas with
It is discharged by chromatography outlet port.
2. gas-chromatography according to claim 1-ion mobility spectrometry detector, which is characterized in that injection port be shunting or
Splitless injecting samples mouth.
3. gas-chromatography according to claim 1-ion mobility spectrometry detector, which is characterized in that chromatographic column is capillary color
It further includes chromatography column sleeve to compose column or boundling capillary column, gas-chromatography mechanism, for protecting chromatographic column and being evenly heated to chromatographic column,
And chromatography column sleeve makes chromatographic column and injection port and is tightly connected between migration tube.
4. gas-chromatography according to claim 1-ion mobility spectrometry detector, which is characterized in that migration tube includes holotype
Formula pipe and negative mode pipe, and be connected to by connector.
5. gas-chromatography according to claim 1-ion mobility spectrometry detector, which is characterized in that connector further includes resistance to
High-temperature insulation disk is set to the both sides of metal terminal pad, and metal terminal pad is grounded.
6. gas-chromatography according to claim 1-ion mobility spectrometry detector, which is characterized in that chromatography metal dish, ion
It migrates metal dish and semi-permeable membrane to fix using O-ring seals and screw assemblies sealing, chromatographic sample chamber and Ion transfer sample cavity
For two independent sealed toroidal cavities.
7. gas-chromatography according to claim 3-ion mobility spectrometry detector, which is characterized in that further include heating film, protect
Warm cotton and shielding case, heating film coat injection port, chromatography column sleeve and migration tube;Heat-preservation cotton coats the outside of heating film;Shielding case
It is set between migration tube and heating film.
8. a kind of gas-chromatography-ion mobility spectrometry combination device, which is characterized in that including air-channel system and such as claim 1 to 7
The gas-chromatography-ion mobility spectrometry detector, wherein
Air-channel system includes that chromatography gas circuit, the first migration gas circuit and the second migration gas circuit, chromatography gas circuit are connected to injection port, chromatography
Sample introduction carrier gas can enter chromatographic column via chromatography gas circuit and injection port, a part of sample molecule can through semipermeable membrane to from
In son migration sample cavity;First migration gas circuit both ends respectively with migration tube and;Second migration gas circuit is connected to migration tube, is used for
Migration gas is provided to migration tube;It can be via the first migration gas circuit, the second migration gas by the migration tube discharge gas of migration tube discharge
Road and Ion transfer sample introduction carrier gas inlet enter transference tube, and are penetrated into Ion transfer sample cavity by chromatographic sample chamber
Sample can enter ionization in migration tube via sample feeding mouth under the action of migrating sample introduction carrier gas, and in the work of migration electric field
It is detected with lower arrival Faraday plate.
9. gas-chromatography-ion mobility spectrometry combination device according to claim 8, which is characterized in that chromatography gas circuit includes
Filter, combination valve and flow controller, chromatography column feed materials carrier gas can via filter, combination valve and flow controller enter into
Sample mouth.
10. gas-chromatography-ion mobility spectrometry combination device according to claim 8, which is characterized in that migration tube includes just
Pattern pipe, negative mode pipe, positive discharge gas interface and negative discharge gas interface, holotype pipe are connected to negative mode pipe by connector,
Positive discharge gas interface is connected to holotype pipe, and negative discharge gas interface is connected to negative mode pipe;Air-channel system further includes buffering bottom plate,
It includes the first cushion chamber and the second cushion chamber to buffer bottom plate, and the first cushion chamber is connected to positive discharge gas interface and the first migration gas circuit
Between, the second cushion chamber is connected between negative discharge gas interface and the first migration gas circuit.
11. gas-chromatography-ion mobility spectrometry combination device according to claim 10, which is characterized in that the first migration gas
Road includes the first branch, the second branch and the third branch connected by threeway, from the first cushion chamber and the second cushion chamber
Migration sample introduction carrier gas converges in the first branch, and the second branch is equipped with molecular sieve, and is connected to Ion transfer sample introduction carrier gas inlet,
Third branch road is equipped with clarifier and miillpore filter, and a part for the migration sample introduction carrier gas from the first branch enters second
Road, another part enter third branch.
12. gas-chromatography-ion mobility spectrometry combination device according to claim 11, which is characterized in that buffering bottom plate packet
It further includes third cushion chamber to include, and the first migration gas circuit further includes the 4th branch, and the second branch is connect with third cushion chamber, the 4th
Road is connected to third cushion chamber and Ion transfer sample introduction carrier gas inlet, and the 4th road is equipped with flow controller.
13. gas-chromatography-ion mobility spectrometry combination device according to claim 12, which is characterized in that the second migration gas
Road includes holotype branch and negative mode branch, and holotype branch is connected between third cushion chamber and holotype pipe, negative mode
Branch is connected between third cushion chamber and negative mode pipe.
14. gas-chromatography-ion mobility spectrometry combination device according to claim 8, which is characterized in that further include circuit,
Circuit includes power module, mainboard, preceding amplification module, high-pressure modular, heating module and control module, and mainboard is used for connection migration pipe
Outgoing cable, and for providing slot for preceding amplification module, high-pressure modular, control panel;Preceding amplification module is for connecing Faraday plate
The signal of receipts carries out shaping, filtering and amplification;High-pressure modular is used to for ion gate provide saltus step pulse, is migration area and is
Grid-disk provides electric field;Heating module is for being heated;Control module is for realizing to heating and gas-chromatography-Ion transfer
Compose the modification and control of detector start and stop.
15. gas-chromatography-ion mobility spectrometry combination device according to claim 8, which is characterized in that further include that shielding is outer
Shell heats shielding shell, Faraday plate shielding cylinder, migration tube bulk shielding shell and high pressure it includes migration tube and preceding puts
Shield shell.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN107907622A (en) * | 2017-12-29 | 2018-04-13 | 同方威视技术股份有限公司 | Gas-chromatography ion mobility spectrometry detector and combined apparatus |
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2017
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107907622A (en) * | 2017-12-29 | 2018-04-13 | 同方威视技术股份有限公司 | Gas-chromatography ion mobility spectrometry detector and combined apparatus |
GB2571428A (en) * | 2017-12-29 | 2019-08-28 | Nuctech Co Ltd | Gas chromatography-ion mobility spectrometry detector and gas chromatograph-ion mobility spectrometer |
GB2571428B (en) * | 2017-12-29 | 2020-05-13 | Nuctech Co Ltd | GC-IMS interface comprising semi-permeable membrane for blocking transmission |
US10989689B2 (en) | 2017-12-29 | 2021-04-27 | Nuctech Company Limited | Gas chromatography-ion mobility spectrometry detector and gas chromatograph-ion mobility spectrometer |
CN107907622B (en) * | 2017-12-29 | 2024-01-23 | 同方威视技术股份有限公司 | Gas chromatograph-ion mobility spectrometry detector and combined device |
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